Hochdrucksynthese und Kristallstruktur von Nd4Au2O9 und Gd4Au2O9 / High Pressure Synthesis and Crystal Structure of Nd4Au2O9 and Gd4Au2O9

1996 ◽  
Vol 51 (6) ◽  
pp. 811-816 ◽  
Author(s):  
Claudia Steiner ◽  
Martina Andratschke ◽  
Klaus-Jürgen Range

Abstract Single crystals of Nd4Au2O9 and Gd4Au2O9 have been prepared by oxidizing mixtures of gold metal and Nd2O3 or Gd2O3, rsp., with KO2 under high-pressure high-temperature conditions (40 kbar, 1200°C) in a modified Belt-type apparatus. The X-ray structure analyses have been carried out on twinned crystals. The compounds crystallize in the orthorhombic space group Pbcn (Nd4Au,O9: a = 11.938(7) ,b = 6.126(2),c = 11.928(3) A ,Z = 4,1 = 0.0443; Gd4Au2O9: a = 11.922(2), 6 = 6.1242(7), c = 11.917(2) A, Z = 4. R1 =0.0232). The title compounds are isostructural with La4Au2O9. Their structure comprises isolated square-planar AuO4 groups, stacked along [010] to form a columnar structure. The Au-Au distance along the columnar direction is 3.10 Å. Structural relations to Bi2CuO4 und (Nd, Pr)2AuO5 are discussed

2017 ◽  
Vol 72 (1) ◽  
pp. 69-76 ◽  
Author(s):  
Daniela Vitzthum ◽  
Michael Schauperl ◽  
Klaus R. Liedl ◽  
Hubert Huppertz

AbstractOrthorhombic In3B5O12 was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 12.2 GPa and 1500°C. Its structure is isotypic to the rare earth analogs RE3B5O12 (RE=Sc, Er–Lu). In the field of indium borate chemistry, In3B5O12 is the third known ternary indium borate besides InBO3 and InB5O9. The crystal structure of In3B5O12 has been determined via single-crystal X-ray diffraction data collected at room temperature. It crystallizes in the orthorhombic space group Pmna with the lattice parameters a=12.570(2), b=4.5141(4), c=12.397(2) Å, and V=703.4(2) Å3. IR and Raman bands of In3B5O12 were theoretically determined and assigned to experimentally recorded spectra.


2020 ◽  
Vol 75 (6-7) ◽  
pp. 589-595
Author(s):  
Birgit Fuchs ◽  
Robert O. Kindler ◽  
Gunter Heymann ◽  
Hubert Huppertz

Abstractγ-Sm(BO2)3 was obtained via a high-pressure/high-temperature approach in a multi-anvil apparatus at 10 GPa and 1673 K. It crystallizes in the orthorhombic space group Pca21 (no. 29) with the lattice parameters a = 18.3088(8), b = 4.4181(2), and c = 4.2551(2) Å. The compound was analysed by means of X-ray diffraction and vibrational spectroscopy. The structure is isotypic to that of the already known meta-oxoborates γ-RE(BO2)3 (RE = La−Nd) and built up of a highly condensed borate framework containing three-, four-, six-, and ten-membered rings. Next to neodymium, samarium represents the second rare earth element that forms the α-, β-, and γ-modification of the four known rare earth meta-oxoborate structure types.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


2008 ◽  
Vol 63 (6) ◽  
pp. 713-717 ◽  
Author(s):  
Almut Haberer ◽  
Hubert Huppertz

The vanadium orthoborate VBO3 was synthesized under high-pressure / high-temperature conditions of 7.5 GPa and 1250 °C in a Walker-type multianvil apparatus. The crystal structure was determined on the basis of single crystal X-ray diffraction data, collected at r. t. The title compound crystallizes in the trigonal calcite structure, space group R3̄c, with the lattice parameters a = 462.0(1) and c = 1450.9(3) pm. Within the trigonal planar BO3 groups, the B-O distance is 138.8(3) pm. The vanadium atoms have a slightly distorted octahedral oxygen coordination (V-O: 202.3(2) pm).


2020 ◽  
Vol 75 (11) ◽  
pp. 975-981
Author(s):  
Daniela Vitzthum ◽  
Ingo Widmann ◽  
Markus Plank ◽  
Bastian Joachim-Mrosko ◽  
Hubert Huppertz

AbstractOrthorhombic HP-Al2B3O7(OH) was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 12.4 GPa and 1200 °C, respectively. Its structure is isotypic to that of Ga2B3O7(OH) and has been determined via single-crystal X-ray diffraction at room temperature. HP-Al2B3O7(OH) crystallizes in the space group Cmce (Z = 8) with the lattice parameters a = 10.3124(4), b = 7.3313(3), c = 10.4801(5) Å, and V = 792.33(6) Å3. The compound has also been characterized by IR and Raman spectroscopy.


2017 ◽  
Vol 72 (12) ◽  
pp. 977-982 ◽  
Author(s):  
Martin K. Schmitt ◽  
Hubert Huppertz

Abstractα-Y2B4O9 was synthesized in a high-pressure/high-temperature experiment at 12.3 GPa/1020°C. The crystal structure has been determined via single-crystal X-ray diffraction. α-Y2B4O9 is isotypic to the lanthanide borates α-Ln2B4O9 (Ln=Sm–Ho) and crystallizes in the monoclinic space group C2/c (no. 15) with the following lattice parameters: a=25.084(2), b=4.3913(2), c=24.726(2) Å, and β=99.97(1)°. The compound was further characterized via X-ray powder diffraction as well as IR and Raman spectroscopy.


2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.


1993 ◽  
Vol 48 (2) ◽  
pp. 237-239 ◽  
Author(s):  
Klaus-Jürgen Range ◽  
Alexandra Atzesdorfer

AbstractThe title compound was prepared by high-pressure reaction of rhenium metal with technical grade (i.e., Na containing) KO2 in a modified Belt-type apparatus (20 kbar, 1000 °C, 60 min, Au capsule). The amber-coloured crystals are very hygroscopic and decompose rapidly when exposed to air. K3NaRe2O9 crystallizes hexagonally, space group P63/mmc, with a = 6.012(1), c = 14.342(14) Å, c/a = 2.386 and Z = 2. The structure was refined to R = 0.031, Rw = 0.023 for 422 independent, absorption-corrected reflections with l > σ (I). K3NaRe2O9 is isostructural with 6H-BaTiO3, a perowskite variant, and contains Na and Re in octaedral coordination. Two ReO6 octahedra are face-sharing, thus creating a Re2O9 double octahedron with a Re-R e distance of 2.92 Å.


1996 ◽  
Vol 51 (5) ◽  
pp. 747-750 ◽  
Author(s):  
Anja Louzikova ◽  
Klaus-Jürgen Range

Single crystals of calcium aurate(III), CaAu2O4, were obtained by high-pressure treatment of a CaO/Au2O3/KO2 mixture at 40 kbar, 1200 °C in a modified Belt-type apparatus. The crystals are tetragonal, space group I41/a, with a = 5.9868(7), c = 10.043(1) Å, c/a = 1.678 and Z = 4.CaAu2O4 is isostructural with LaPd2O4, SrAu2O4 and BaAu2O4. Its structure comprises square-planar AuO4 groups (< Au-O > = 2.007 Å), which are stacked into columns along [100] and [010], These columns are connected by shared corners forming a three-dimensional framework. The Ca ions are situated in tunnels created by the gold-oxygen partial structure. They are surrounded by eight oxygen atoms (<Ca-O> = 2.490 Å) in a slightly distorted dodecahedron.


2001 ◽  
Vol 56 (8) ◽  
pp. 697-703 ◽  
Author(s):  
Hubert Huppertz

β-Ytterbium borate (β-YbBO3) was synthesized under high-pressure in a Walker-type multianvil apparatus at 2.2 GPa and 1400 °C. The title-compound crystallizes in the trigonal calcite structure, space group R3̄̄c. Single crystal X-ray data yielded a = 492.1(2), c = 1630.5(9) pm, wR2 = 0.0344 for 165 F2 values and 11 variable parameters. Within the trigonal planar BO3 groups the B-O distance is 137.8(4) pm. The ytterbium atoms have a slightly distorted octahedral oxygen coordination (Yb-O: 224.4(2) pm)


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